Search results for: headspace gas chromatography

Authors: Birute Bugelyte, Ingrida Jurkute, Vida Vickackaite

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The most complicated step of the determination of volatile compounds in complex matrices is the separation of analytes from the matrix. Traditional analyte separation methods (liquid extraction, Soxhlet extraction) require a lot of time and labour; moreover, there is a risk to lose the volatile analytes. In recent years, headspace gas chromatography has been used to determine volatile compounds. To date, traditional extraction solvents have been used in headspace gas chromatography. As a rule, such solvents are rather volatile; therefore, a large amount of solvent vapour enters into the headspace together with the analyte. Because of that, the determination sensitivity of the analyte is reduced, a huge solvent peak in the chromatogram can overlap with the peaks of the analyts. The sensitivity is also limited by the fact that the sample can’t be heated at a higher temperature than the solvent boiling point. In 2018 it was suggested to replace traditional headspace gas chromatographic solvents with non-volatile, eco-friendly, biodegradable, inexpensive, and easy to prepare deep eutectic solvents (DESs). Generally, deep eutectic solvents have low vapour pressure, a relatively wide liquid range, much lower melting point than that of any of their individual components. Those features make DESs very attractive as matrix media for application in headspace gas chromatography. Also, DESs are polar compounds, so they can be applied for microwave assisted extraction. The aim of this work was to investigate the possibility of applying deep eutectic solvents for microwave assisted extraction and headspace gas chromatographic determination of hexanal in fat-rich food. Hexanal is considered one of the most suitable indicators of lipid oxidation degree as it is the main secondary oxidation product of linoleic acid, which is one of the principal fatty acids of many edible oils. Eight hydrophilic and hydrophobic deep eutectic solvents have been synthesized, and the influence of the temperature and microwaves on their headspace gas chromatographic behaviour has been investigated. Using the most suitable DES, microwave assisted extraction conditions and headspace gas chromatographic conditions have been optimized for the determination of hexanal in potato chips. Under optimized conditions, the quality parameters of the prepared technique have been determined. The suggested technique was applied for the determination of hexanal in potato chips and other fat-rich food.

Keywords: deep eutectic solvents, headspace gas chromatography, hexanal, microwave assisted extraction

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Authors: Alexandre Gonzalez, Zohra Benfodda, David Bénimélis, Jean-Xavier Fontaine, Roland Molinié, Patrick Meffre

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Volatile organic compounds (VOCs) emitted by flowers play an important role in plant ecology. However, the Tillandsia genus has been scarcely studied according to the VOCs emitted by flowers. Tillandsia are epiphytic flowering plants belonging to the Bromeliaceae family. The VOCs composition of twelve unscented and two faint-scented Tillandsia species was studied. The headspace solid phase microextraction coupled with gas chromatography combined with mass spectrometry method was used to explore the chemical diversity of the VOCs. This study allowed the identification of 65 VOCs among the fourteen species, and between six to twenty-five compounds were identified in each of the species.

Keywords: tillandsia, headspace solid phase microextraction (HS-SPME), gas chromatography-mass spectrometry (GC-MS), scentless flowers, volatile organic compounds (VOCs), PCA analysis, heatmap

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Authors: Kooshan Nayebzadeh, Maryam Enteshari, Abdorreza Mohammadi

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The oxidative stability of mayonnaise under different storage temperatures (4 and 25˚C) during 6-month shelf-life was investigated by different analytical methods. In this study, headspace single-drop microextarction (HS-SDME) combined with gas chromatography-mass spectrometry (GC-MS) as a green, sensitive and rapid technique was applied to evaluate oxidative state in mayonnaise. Oxidation changes of extracted oil from mayonnaise were monitored by analytical parameters including peroxide value (PV), p-Anisidine value (p-An V), thiobarbituric acid value (TBA), and oxidative stability index (OSI). Hexanal and heptanal as secondary volatile oxidation compounds were determined by HS-SDME/GC-MS method in mayonnaise matrix. The rate of oxidation in mayonnaises increased during storage and it was determined greater at 25 ˚C. The values of Anisidine and TBA were gradually enhanced during 6 months, while the amount of OSI decreased. At both temperatures, the content of hexanal was higher than heptanal during all storage periods. Also significant increments in hexanal and heptanal concentrations in the second and sixth month of storage have been observed. Hexanal concentrations in mayonnaises which were stored at 25 ˚C and during storage time showed the highest values. It can be concluded that the temperature and duration of storage time are definitive parameters which affect on quality and oxidative stability of mayonnaise. Additionally, hexanal content in comparison to heptanal is a more reliable oxidative indicator and HS-SDME/GC-MS can be applied in a quick and simple manner.

Keywords: oxidative stability, mayonnaise, headspace single-drop microextarction (HS-SDME), shelf-life

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Authors: Maryam Enteshari, Kooshan Nayebzadeh, Abdorreza Mohammadi

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In this study, the oxidative stability of soybean oil under different storage temperatures (4 and 25˚C) and during 6-month shelf-life was investigated by various analytical methods and headspace-liquid phase microextraction (HS-LPME) coupled to gas chromatography-mass spectrometry (GC-MS). Oxidation changes were monitored by analytical parameters consisted of acid value (AV), peroxide value (PV), p-Anisidine value (p-AV), thiobarbituric acid value (TBA), fatty acids profile, iodine value (IV), and oxidative stability index (OSI). In addition, concentrations of hexanal and heptanal as secondary volatile oxidation compounds were determined by HS-LPME/GC-MS technique. Rate of oxidation in soybean oil which stored at 25˚C was so higher. The AV, p-AV, and TBA were gradually increased during 6 months while the amount of unsaturated fatty acids, IV, and OSI decreased. Other parameters included concentrations of both hexanal and heptanal, and PV exhibited increasing trend during primitive months of storage; then, at the end of third and fourth months a sudden decrement was understood for the concentrations of hexanal and heptanal and the amount of PV, simultaneously. The latter parameters increased again until the end of shelf-time. As a result, the temperature and time were effective factors in oxidative stability of soybean oil. Also intensive correlations were found for soybean oil at 4 ˚C between AV and TBA (r2=0.96), PV and p-AV (r2=0.9), IV and TBA (-r2=0.9), and for soybean oil stored at 4˚C between p-AV and TBA (r2=0.99).

Keywords: headspace-liquid phase microextraction, oxidation, shelf-life, soybean oil

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Authors: Ali Ammari, Karin Schroen

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In brewing industries, stripping is a downstream process to separate volatiles from beer. Due to physiochemical similarities between flavour components, the selectivity of this method is not favourable. Besides, the presence of non-volatile compounds such as proteins and carbohydrates may affect the separation of flavours due to their retaining properties. By using a stripping column with structured packing coupled with a gas chromatography, in this work, the overall mass transfer coefficient along with their corresponding equilibrium data was investigated for a model solution consist of water, ethanol, ethyl acetate and isoamyl acetate. Static headspace analysis also was employed to derive equilibrium data for flavours in the presence of beer dry matter. As it was expected ethanol and dry matter showed retention properties; however, the effect of viscosity in mass transfer coefficient was discarded due to the fact that the viscosity of solution decreased during stripping. The effect of ethanol and beer dry matter were mapped to be used for designing stripping could.

Keywords: flavour, headspace, Henry’s coefficient, mass transfer coefficient, stripping

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Authors: K. Mohammed, M. Agarwal, J. Mewman, Y. Ren

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An optimum technic has been developed for extracting volatile organic compounds which contribute to the aroma of lime fruit (Citrus aurantifolia). The volatile organic compounds of healthy and infested lime fruit with California red scale Aonidiella aurantii were characterized using headspace solid phase microextraction (HS-SPME) combined with gas chromatography (GC) coupled flame ionization detection (FID) and gas chromatography with mass spectrometry (GC-MS) as a very simple, efficient and nondestructive extraction method. A three-phase 50/30 μm PDV/DVB/CAR fibre was used for the extraction process. The optimal sealing and fibre exposure time for volatiles reaching equilibrium from whole lime fruit in the headspace of the chamber was 16 and 4 hours respectively. 5 min was selected as desorption time of the three-phase fibre. Herbivorous activity induces indirect plant defenses, as the emission of herbivorous-induced plant volatiles (HIPVs), which could be used by natural enemies for host location. GC-MS analysis showed qualitative differences among volatiles emitted by infested and healthy lime fruit. The GC-MS analysis allowed the initial identification of 18 compounds, with similarities higher than 85%, in accordance with the NIST mass spectral library. One of these were increased by A. aurantii infestation, D-limonene, and three were decreased, Undecane, α-Farnesene and 7-epi-α-selinene. From an applied point of view, the application of the above-mentioned VOCs may help boost the efficiency of biocontrol programs and natural enemies’ production techniques.

Keywords: lime fruit, Citrus aurantifolia, California red scale, Aonidiella aurantii, VOCs, HS-SPME/GC-FID-MS

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Authors: A. Mandić, M. Sakač, A. Mišan, B. Šojić, L. Petrović, I. Lončarević, B. Pajin, I. Sedej

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Aldehydes as secondary lipid oxidation products are highly specific to the oxidative degradation of particular polyunsaturated fatty acids present in foods. Gas chromatographic analysis of those volatile compounds has been widely used for monitoring of the deterioration of food products. Developed static headspace gas chromatography method using flame ionization detector (SHS GC FID) was applied to monitor the aldehydes present in processed foods such as bakery, meat and confectionary products. Five selected aldehydes were determined in samples without any sample preparation, except grinding for bakery and meat products. SHS–GC analysis allows the separation of propanal, pentanal, hexanal, heptanal and octanal, within 15min. Aldehydes were quantified in fresh and stored samples, and the obtained range of aldehydes in crackers was 1.62±0.05-9.95±0.05mg/kg, in sausages 6.62±0.46-39.16±0.39mg/kg; and in cocoa spread cream 0.48±0.01-1.13±0.02mg/kg. Referring to the obtained results, the following can be concluded, proposed method is suitable for different types of samples, content of aldehydes varies depending on the type of a sample, and differs in fresh and stored samples of the same type.

Keywords: lipid oxidation, aldehydes, crackers, sausage, cocoa cream spread

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Authors: Kooshan Nayebzadeh, Maryam Enteshari

Abstract:

In this study, the oxidative stability of soybean oil under different storage temperatures (4 and 25 ˚C) and during 6-month shelf-life was investigated by various analytical methods and headspace-liquid phase microextraction (HS-LPME) coupled to gas chromatography-mass spectrometry (GC-MS). Oxidation changes were monitored by analytical parameters consisted of acid value (AV), peroxide value (PV), p-Anisidine value (p-AV), thiobarbituric acid value (TBA), fatty acids profile, iodine value (IV) and oxidative stability index (OSI). In addition, concentrations of hexanal and heptanal as secondary volatile oxidation compounds were determined by HS-LPME/GC-MS technique. Rate of oxidation in soybean oil which stored at 25 ˚C was so higher. The AV, p-AV, and TBA were gradually increased during 6 months, while the amount of unsaturated fatty acids, IV, and OSI decreased. Other parameters included concentrations of both hexanal and heptanal, and PV exhibited increasing trend during primitive months of storage; then, at the end of third and fourth months a sudden decrement was understood for the concentrations of hexanal and heptanal and the amount of PV, simultaneously. The latter parameters increased again until the end of shelf-time. As a result, the temperature and time were effective factors in oxidative stability of soybean oil. Also intensive correlations were found for soybean oil at 4 ˚C between AV and TBA (r2=0.96), PV and p-AV (r2=0.9), IV and TBA (-r2=0.9), and for soybean oil stored at 4 ˚C between p-AV and TBA (r2=0.99).

Keywords: headspace-liquid phase microextraction, oxidation, shelf-life, soybean oil

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Authors: Igor Jerkovic

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Biodiversity of flora provides many different nectar sources for the bees. Unifloral honeys possess distinctive flavours, mainly derived from their nectar sources (characteristic volatile organic components (VOCs)). Specific or nonspecific VOCs (chemical markers) could be used for unifloral honey characterisation as addition to the melissopalynologycal analysis. The main honey volatiles belong, in general, to three principal categories: terpenes, norisoprenoids, and benzene derivatives. Some of these substances have been described as characteristics of the floral source, and other compounds, like several alcohols, branched aldehydes, and furan derivatives, may be related to the microbial purity of honey processing and storage conditions. Selection of the extraction method for the honey volatiles profiling should consider that heating of the honey produce different artefacts and therefore conventional methods of VOCs isolation (such as hydrodistillation) cannot be applied for the honey. Two-way approach for the isolation of the honey VOCs was applied using headspace solid-phase microextraction (HS-SPME) and ultrasonic solvent extraction (USE). The extracts were analysed by gas chromatography and mass spectrometry (GC-MS). HS-SPME (with the fibers of different polarity such as polydimethylsiloxane/ divinylbenzene (PDMS/DVB) or divinylbenzene/carboxene/ polydimethylsiloxane (DVB/CAR/PDMS)) enabled isolation of high volatile headspace VOCs of the honey samples. Among them, some characteristic or specific compounds can be found such as 3,4-dihydro-3-oxoedulan (in Centaurea cyanus L. honey) or 1H-indole, methyl anthranilate, and cis-jasmone (in Citrus unshiu Marc. honey). USE with different solvents (mainly dichloromethane or the mixture pentane : diethyl ether 1 : 2 v/v) enabled isolation of less volatile and semi-volatile VOCs of the honey samples. Characteristic compounds from C. unshiu honey extracts were caffeine, 1H-indole, 1,3-dihydro-2H-indol-2-one, methyl anthranilate, and phenylacetonitrile. Sometimes, the selection of solvent sequence was useful for more complete profiling such as sequence I: pentane → diethyl ether or sequence II: pentane → pentane/diethyl ether (1:2, v/v) → dichloromethane). The extracts with diethyl ether contained hydroquinone and 4-hydroxybenzoic acid as the major compounds, while (E)-4-(r-1’,t-2’,c-4’-trihydroxy-2’,6’,6’-trimethylcyclo-hexyl)but-3-en-2-one predominated in dichloromethane extracts of Allium ursinum L. honey. With this two-way approach, it was possible to obtain a more detailed insight into the honey volatile and semi-volatile compounds and to minimize the risks of compound discrimination due to their partial extraction that is of significant importance for the complete honey profiling and identification of the chemical biomarkers that can complement the pollen analysis.

Keywords: honey chemical biomarkers, honey volatile compounds profiling, headspace solid-phase microextraction (HS-SPME), ultrasonic solvent extraction (USE)

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Authors: A. Ramachandra Reddy, V. Murugan, Prema Kumari

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Residual solvents in Pharmaceutical samples are monitored using gas chromatography with headspace (GC-HS). Based on current regulatory and compendial requirements, measuring the residual solvents are mandatory for all release testing of active pharmaceutical ingredients (API). Generally, isopropyl alcohol is used as the residual solvent in proline and tryptophan; methanol in cysteine monohydrate hydrochloride, glycine, methionine and serine; ethanol in glycine and lysine monohydrate; acetic acid in methionine. In order to have a single method for determining these residual solvents (isopropyl alcohol, ethanol, methanol and acetic acid) in all these 7 amino acids a sensitive and simple method was developed by using gas chromatography headspace technique with flame ionization detection. During development, no reproducibility, retention time variation and bad peak shape of acetic acid peaks were identified due to the reaction of acetic acid with the stationary phase (cyanopropyl dimethyl polysiloxane phase) of column and dissociation of acetic acid with water (if diluent) while applying temperature gradient. Therefore, dimethyl sulfoxide was used as diluent to avoid these issues. But most the methods published for acetic acid quantification by GC-HS uses derivatisation technique to protect acetic acid. As per compendia, risk-based approach was selected as appropriate to determine the degree and extent of the validation process to assure the fitness of the procedure. Therefore, Total error concept was selected to validate the analytical procedure. An accuracy profile of ±40% was selected for lower level (quantitation limit level) and for other levels ±30% with 95% confidence interval (risk profile 5%). The method was developed using DB-Waxetr column manufactured by Agilent contains 530 µm internal diameter, thickness: 2.0 µm, and length: 30 m. A constant flow of 6.0 mL/min. with constant make up mode of Helium gas was selected as a carrier gas. The present method is simple, rapid, and accurate, which is suitable for rapid analysis of isopropyl alcohol, ethanol, methanol and acetic acid in amino acids. The range of the method for isopropyl alcohol is 50ppm to 200ppm, ethanol is 50ppm to 3000ppm, methanol is 50ppm to 400ppm and acetic acid 100ppm to 400ppm, which covers the specification limits provided in European pharmacopeia. The accuracy profile and risk profile generated as part of validation were found to be satisfactory. Therefore, this method can be used for testing of residual solvents in amino acids drug substances.

Keywords: amino acid, head space, gas chromatography, total error

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Authors: Igor Jerkovic

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Owing to the attractive sensory properties and low odour thresholds, norisoprenoids (degraded carotenoid-like structures with 3,5,5-trimethylcyclohex-2-enoic unit) have been identified as aroma contributors in a number of different matrices. C₁₃-Norisoprenoids have been found among volatile organic compounds of various honey types as well as C₉//C₁₀-norisoprenoids or C₁₄/C₁₅-norisoprenoids. Besides degradation of abscisic acid (which produces, e.g., dehydrovomifoliol, vomifoliol, others), the cleavage of the C(9)=C(10) bond of other carotenoid precursors directly generates nonspecific C₁₃-norisoprenoids such as trans-β-damascenone, 3-hydroxy-trans-β-damascone, 3-oxo-α-ionol, 3-oxo-α-ionone, β-ionone found in various honey types. β-Damascenone and β-ionone smelling like honey, exhibit the lowest odour threshold values of all C₁₃-norisoprenoids. The presentation is targeted on two uncommon C₁₃-norisoprenoids in the honey flavor that could be used as specific or nonspecific chemical markers of the botanical origin. Namely, after screening of different honey types, the focus was directed on Centaruea cyanus L. and Allium ursinum L. honey. The samples were extracted by headspace solid-phase microextraction (HS-SPME) and ultrasonic solvent extraction (USE) and the extracts were analysed by gas chromatography and mass spectrometry (GC-MS). SPME fiber with divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) coating was applied for the research of C. cyanus honey headspace and predominant identified compound was 3,4-dihydro-3-oxoedulan (2,5,5,8a-tetramethyl-2,3,5,6,8,8a-hexahydro-7H-chromen-7-one also known as 2,3,5,6,8,8a-hexahydro-2,5,5,8a-tetramethyl-7H-1-benzo-pyran-7-one). The oxoedulan structure contains epoxide and it is more volatile in comparison with its hydroxylated precursors. This compound has not been found in other honey types and can be considered specific for C. cyanus honey. The dichloromethane extract of A. ursinum honey contained abundant (E)-4-(r-1',t-2',c-4'-trihydroxy-3',6',6'-trimethylcyclohexyl)-but-3-en-2-one that was previously isolated as dominant substance from the ether extracts of New Zealand thyme honey. Although a wide variety of degraded carotenoid-like substances have been identified from different honey types, this appears to be rare situation where 3,4-dihydro-3-oxoedulan and (E)-4-(r-1',t-2',c-4'-trihydroxy-3',6',6'-trimethylcyclohexyl)-but-3-en-2-one have been found that is of great importance for chemical fingerprinting and identification of the chemical biomarkers that can complement the pollen analysis as the major method for the honey classification.

Keywords: 3, 4-dihydro-3-oxoedulan, (E)-4-(r-1', t-2', c-4'-trihydroxy-3', 6', 6'-trimethylcyclohexyl)-but-3-en-2-one, honey flavour, C₁₃-norisoprenoids

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Authors: M. O. Ezegbogu, H. B. Osadolor

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Lipsticks constitute a significant source of transfer evidence, and can, therefore, provide corroborative or inclusionary evidence in criminal investigation. This study aimed to determine the uniqueness and persistence of different lipstick smears using Thin Layer Chromatography (TLC), and Gas Chromatography with a Flame Ionisation Detector (GC-FID). In this study, we analysed lipstick smears retrieved from tea cups exposed to the environment for up to four weeks. The n-alkane content of each sample was determined using GC-FID, while TLC was used to determine the number of bands, and retention factor of each band per smear. This study shows that TLC gives more consistent results over a 4-week period than GC-FID. It also proposes a maximum exposure time of two weeks for the analysis of lipsticks left in the open using GC-FID. Finally, we conclude that neither TLC nor GC-FID can distinguish lipstick evidence recovered from hypothetical crime scenes.

Keywords: forensic science, chromatography, identification, lipstick

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Authors: Lorenzo Cocola, Massimo Fedel, Dragiša Savić, Bojana Danilović, Luca Poletto

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An instrument for the detection and evaluation of gaseous carbon dioxide in the headspace of closed containers has been developed in the context of Packsensor Italian-Serbian joint project. The device is based on Tunable Diode Laser Absorption Spectroscopy (TDLAS) with a Wavelength Modulation Spectroscopy (WMS) technique in order to accomplish a non-invasive measurement inside closed containers of fermented dairy products (yogurts and fermented cheese in cups and bottles). The purpose of this instrument is the continuous monitoring of carbon dioxide concentration during incubation and storage of products over a time span of the whole shelf life of the product, in the presence of different microorganisms. The instrument’s optical front end has been designed to be integrated in a thermally stabilized incubator. An embedded computer provides processing of spectral artifacts and storage of an arbitrary set of calibration data allowing a properly calibrated measurement on many samples (cups and bottles) of different shapes and sizes commonly found in the retail distribution. A calibration protocol has been developed in order to be able to calibrate the instrument on the field also on containers which are notoriously difficult to seal properly. This calibration protocol is described and evaluated against reference measurements obtained through an industry standard (sampling) carbon dioxide metering technique. Some sets of validation test measurements on different containers are reported. Two test recordings of carbon dioxide concentration evolution are shown as an example of instrument operation. The first demonstrates the ability to monitor a rapid yeast growth in a contaminated sample through the increase of headspace carbon dioxide. Another experiment shows the dissolution transient with a non-saturated liquid medium in presence of a carbon dioxide rich headspace atmosphere.

Keywords: TDLAS, carbon dioxide, cups, headspace, measurement

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Authors: Thamer Alshuwaili, Yonglin Ren, Bob Du, Manjree Agarwal

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The warehouse beetle, Trogoderma variabile Ballion (Coleoptera: Dermestidae), is a major pest of packaged and processed stored products. Warehouse beetle is the common name which was given by Okumura (1972). This pest has been reported to infest 119 different commodities, and it is distributed throughout the tropical and subtropical parts of the world. Also, it is difficult to control because of the insect's ability to stay without food for long times, and it can survive for years under dry conditions and low-moisture food, and it has also developed resistance to many insecticides. The young larvae of these insects can cause damage to seeds, but older larvae prefer to feed on whole grains. The percentage of damage caused by these insects range between 30-70% in the storage. T. variabile is the species most responsible for causing significant damage in grain stores worldwide. Trogoderma spp. is a huge problem for cereal grains, and there are many countries, such as the USA, Australia, China, Kenya, Uganda and Tanzania who have specific quarantine regulations against possible importation. Also, grain stocks can be almost completely destroyed because of the massive populations the insect may develop. However, the purpose of the current research was to optimize conditions to collect volatile organic compound from Trogoderma variabile at different life stages by using headspace solid phase microextraction (SPME) coupled with gas chromatography-mass spectrometry (GC-MS) and flame ionization detection (FID). Using SPME technique to extract volatile from insects is an efficient, straightforward and nondestructive method. Result of the study shows that 15 insects were optimal number for larvae and adults. Selection of the number of insects depend on the height of the peak area and the number of peaks. Sixteen hours were optimized as the best extraction time for larvae and 8 hours was the optimal number of adults.

Keywords: Trogoderma variabile, warehouse beetle , GC-MS, Solid phase microextraction

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Authors: Evgeny E. Tereshatov

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Astatine-211 is considered one of the most promising radionuclides for Targeted Alpha Therapy. In order to develop reliable procedures to label biomolecules and utilize efficient delivery vehicle principles, one should understand the main chemical characteristics of astatine. The short half-life of 211At (~7.2 h) and absence of any stable isotopes of this element are limiting factors towards studying the behavior of astatine. Our team has developed a procedure for rapid and efficient isolation of astatine from irradiated bismuth material in nitric acid media based on 3-octanone and 1-octanol extraction chromatography resins. This process has been automated and it takes 20 min from the beginning of the target dissolution to the At-211 fraction elution. Our next step is to consider commercially available chromatography resins and their applicability in astatine purification in the same media. Results obtained along with the corresponding sorption mechanisms will be discussed.

Keywords: astatine-211, chromatography, automation, mechanism, radiopharmaceuticals

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Authors: Cristina Munoz-Shuguli, Francisco Rodriguez, Julio Bruna, M. Jose Galotto, Abel Guarda

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The microbial contamination in fruits due to the presence of fungal is the most important cause of their deterioration and loss. The development of active food packaging materials with antifungal properties has been proposed as an innovative strategy in order to prevent this problem. In this way, natural compounds as the essential oils or their derivatives, also called volatile compounds (VC), can be incorporated in the food packaging materials to control the fungal growth during fruit packaging. However, if the VC is incorporated directly in the packaging material, it is released very fast due to VC high volatility. For this reason, the formation of inclusion complexes through the encapsulation of VC into beta-cyclodextrin (β-CD) and their incorporation in package materials is an alternative to maintain an antifungal atmosphere around the packaged fruits for longer times. In this context, the aim of this work was to develop inclusion complexes based in β-CD and VC (β-CD:VC) for further application in the antifungal food packaging materials development. β-CD:VC inclusion complexes were obtained with two different molar ratios 2:1 and 1:1, through co-precipitation method. The entrapment efficiency of β-CD:VC as well the release of antifungal compound from inclusion complexes exposed to different relative humidity (25, 50, and 97 %) to headspace were determined by gaseous chromatography (GC). Also, thermal and antimicrobial properties of β-CD:VC were determined through thermogravimetric analysis (TGA) and antifungal assays against Botrytis cinerea, respectively. GC results showed that β-CD:VC 2:1 had a higher entrapment efficiency than β-CD:VC 1:1, with values of 75.5 ± 3.71 % and 59.6 ± 1.51 %, respectively. It was probably because during the synthesis of β-CD:VC 1:1, there was less molecular space to the movement of VC molecules. Furthermore, the release of VC from β-CD:VC was directly related with the relative humidity. High amount of VC was released when the inclusion complexes were exposed to high humidity, possibly due to the interactions between the water molecules and the β-CD hydrophilic wall. On the other hand, a better thermal stability of VC in inclusion complexes allowed to verify its effective encapsulation into β-CD. Finally, antimicrobial assays showed that the inclusion complexes had a high antifungal activity at very low concentrations. Therefore, the results obtained in this work allow suggesting the β-CD:VC inclusion complexes as potential candidates to the development of fruit antifungal packaging materials, which activity is relative humidity dependent.

Keywords: Botrytis cinerea, fruit packaging, headspace release, volatile compounds

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Authors: Liping Qiu, Xiaofeng Zhang

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The ion chromatography method for the rapid determination of four anions (F⁻、Cl⁻、SO₄²⁻、NO₃⁻) in burial ground poles was optimized. The L₉(₃⁴) orthogonal test was used to determine the optimal parameters of sample pretreatment: accurately weigh 2.000g of sample, add 10mL of ultrapure water, and extract for 40min under the conditions of shaking temperature 40℃ and shaking speed 180 r·min-1. The eluent was 25 mmol/L KOH solution, the analytical column was Ion Pac® AS11-SH (250 mm × 4.0 mm), and the purified filtrate was measured by a conductivity detector. Under this method, the detection limit of each ion is 0.066～0.078mg/kg, the relative standard deviation is 0.86%～2.44% (n=7), and the recovery rate is 94.6～101.9.

Keywords: ion chromatography, tomb, anion (F⁻, Cl⁻, SO₄²⁻, NO₃⁻), environmental protection

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Authors: A. B. Bazaralieva, A. A. Turgumbayeva

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The phytosubstance from garlic was obtained by extraction with liquid carbon dioxide under critical conditions. Methods of processing raw materials are proposed, and the chemical composition of garlic is studied by gas chromatography and mass spectrometry. The garlic extract's composition was determined using gas chromatography (GC) and gas chromatography-mass spectrophotometry (GC-MS). The phytosubstance had 54 constituents. The extract included the following main compounds: Manool (39.56%), Viridifrolol (7%), Podocarpa-1,8,11,13-tetraen-3-one, 14-isopropyl-1,13-dimethoxy- 5,15 percent, (+)-2-Bornanone (4.29%), Thujone (3.49%), Linolic acid ethyl ester (3.41%), and 12-O-Methylcarn.

Keywords: Allium sativum, bioactive compounds of garlic, carbon dioxide extraction of garlic, GS-MS method

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Authors: Bazaraliyeva Aigerim Bakytzhanovna, Turgumbayeva Aknur Amanbekovna

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The phytosubstance from garlic was obtained by extraction with liquid carbon dioxide under critical conditions. Methods of processing raw materials are proposed, and the chemical composition of garlic is studied by gas chromatography and mass spectrometry. The garlic extract's composition was determined using gas chromatography (GC) and gas chromatography-mass spectrophotometry (GC-MS). The phytosubstance had 54 constituents. The extract included the following main compounds: Manool (39.56%), Viridifrolol (7%), Podocarpa-1,8,11,13-tetraen-3-one, 14-isopropyl-1,13-dimethoxy- 5,15 percent, (+)-2-Bornanone (4.29%), Thujone (3.49%), Linolic acid ethyl ester (3.41%), and 12-O-Methylcarn.

Keywords: allium sativum, bioactive compounds of garlic, carbon dioxide extraction of garlic, GS-MS method

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Authors: Methaq Algabr, Nabil Al-Hajj, Ameerh Jaber, Amtellah Alshotobi, Shaima'a Al-suryhi, Gadah Whaban, Nawal Alshehari

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Steam distillation of the essential oil of P. jaubertii was performed using a Clevenger apparatus. Essential oils were analyzed by gas chromatography-flame ionization detector (GC-FID) and gas chromatography coupled to chromatography–mass spectrometry (GC-MS). The major chemical components identified in P. jaubertii essential oil include carvotanacetone (63.975%), 1-methyl-1,2-propanedione (5.887%), 2,5-dimethoxy-para-cymene (3.303%) and ar-curcumene (3.276%). The antimicrobial activity of the essential oil of P. jaubertii was evaluated against all tested microorganisms. P. jaubertii essential oil inhibited all tested microorganisms except Escherichia coli with a minimum inhibitory concentration (MIC) of 5.0 μg/mL against Staphylococcus aureus.

Keywords: Pulicaria jaubertii, essential oil, antimicrobial, Carvotancetone

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Authors: Noorizal Huang, Christian Girsang, Mohamad Razi Mansoor

Abstract:

Shallow gas seepage was first spotted at a central processing platform offshore Malaysia in 2010, acknowledged as Platform T in this paper. Frequent monitoring of the gas seepage was performed through remotely operated vehicle (ROV) baseline survey and a comprehensive geophysical survey was conducted to understand the characteristics of the gas seepage and to ensure that the integrity of the foundation at Platform T was not compromised. The origin of the gas back then was unknown. A soil investigation campaign was performed in 2016 to study the origin of the gas seepage. Two boreholes were drilled; a composite borehole to 150m below seabed for the purpose of soil sampling and in-situ testing and a pilot hole to 155m below the seabed, which was later converted to a fit-for-purpose relief well as an alternate migration path for the gas. During the soil investigation campaign, dissipation tests were performed at several layers which were potentially the source or migration path for the gas. Five (5) soil samples were segregated for headspace test, to identify the gas type which subsequently can be used to identify the origin of the gas. Dissipation tests performed at four depth intervals indicates pore water pressure less than 20 % of the effective vertical stress and appear to continue decreasing if the test had not been stopped. It was concluded that a low to a negligible amount of excess pore pressure exist in clayey silt layers. Results from headspace test show presence of methane corresponding to the clayey silt layers as reported in the boring logs. The gas most likely comes from biogenic sources, feeding on organic matter in situ over a large depth range. It is unlikely that there are large pockets of gas in the soil due to its homogeneous clayey nature and the lack of excess pore pressure in other permeable clayey silt layers encountered. Instead, it is more likely that when pore water at certain depth encounters a more permeable path, such as a borehole, it rises up through this path due to the temperature gradient in the soil. As the water rises the pressure decreases, which could cause gases dissolved in the water to come out of solution and form bubbles. As a result, the gas will have no impact on the integrity of the foundation at Platform T. The fit-for-purpose relief well design as well as adopting headspace testing can be used to address the shallow gas issue at Platform T in a cost effective and efficient manners.

Keywords: dissipation test, headspace test, excess pore pressure, relief well, shallow gas

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Authors: M. Yakoubi, N. Belboukhari, A. Cheriti, K. Sekoum

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Launaea nudicaulis (L.) Hook.f. is a desert, spontaneous plant and endemic to northem Sahara, which belongs to the Asteraceae family. This species exists in the region of Bechar (Local name; El-Rghamma). In our knowledge, no work has been founded, except studies showing the antimicrobial and antifungal activity of methalonic extract of this plant. The present paper describes the chemical composition of the essential oil from Launaea nudicaulis and qualification of isolation and identification of some pure products by column chromatography. The essential oil from the aerial parts of Launaea nudicaulis (Asteraceae) was obtained by hydroditillation in 0.4% yield, led to isolation of four several new products. The isolation is made by column chromatography and followed by GC-IK and GC-MS analysis.

Keywords: Launaea nudicaulis, asteraceae, essential oil, column chromatography, GC-FID, GC-MS

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Authors: A. D. Susanti, W. B. Sediawan, S. K. Wirawan, Budhijanto, Ritmaleni

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Rice bran oil contains significant amounts of oryzanol, a natural antioxidant that considered has higher antioxidant activity than vitamin E (tocopherol). Oryzanol reviewed has several health properties and interested in pharmacy, nutrition, and cosmetics. For practical usage, isolation and purification would be necessary due to the low concentration of oryzanol in crude rice bran oil (0.9-2.9%). Batch chromatography has proved as a promising process for the oryzanol recovery, but productivity was still low and scale-up processes of industrial interest have not yet been described. In order to improve productivity of batch chromatography, a continuous chromatography design namely Simulated Moving Bed (SMB) concept have been proposed. The SMB concept has interested for continuous commercial scale separation of binary system (oryzanol and rice bran oil), and rice bran oil still obtained as side product. Design of SMB chromatography for oryzanol separation requires quantification of its equilibrium. In this study, equilibrium of oryzanol separation conducted in batch adsorption using silica as the adsorbent and n-hexane/acetone (9:1) as the eluent. Three isotherm models, namely the Henry, Langmuir, and Freundlich equations, have been applied and modified for the experimental data to establish appropriate correlation for each sample. It turned out that the model quantitatively describe the equilibrium experimental data and will directed for design of SMB chromatography.

Keywords: adsorption, equilibrium, oryzanol, rice bran oil, simulated moving bed

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Authors: Preeti Panthari, Harsha Kharkwal

Abstract:

Myrica nagi belongs to Myricaceae family. It is known for its therapeutic use since ancient times. The leaves were extracted with methanol and further fractioned with different solvents with increasing polarity. The n-butanol fraction of methanol extract was passed through celite, on separation through silica gel column chromatography yielded ten fractions. For the first time we report isolation of Caffeic acid from n-butanol fraction of Myrica nagi leaves in Chloroform: methanol (70:30) fraction. The mobile phase used for analysis in HPLC was Methanol: water (60:40) at the flow rate of 1 ml/min at wavelength of 280 nm. The retention time was 2.66 mins.

Keywords: Myrica nagi, column chromatography, retention time, caffeic acid

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Authors: Totik Sri Mariani, Sukrasno Isna, Tet Fatt Chia

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Purwoceng (Pimpinella pruatjan Molk) is a legend plant used for increasing stamina by Kings in Java Island, Indonesia. Purpose of this study was to perform meristem culture and detected its stigmasterol by thin layer chromatography (TLC). Our result show that meristem culture could be propagated and grew into plantlet. After extracting intact acclimatized plant derived from meristem culture by hexane, we could detected stigmasterol by TLC. For suggestion, our extraction and TLC method could be used for detecting stigmasterol in others plant.

Keywords: purwoceng (pimpinella pruatjan), meristem culture, extraction, thin layer chromatography

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Authors: Fairouz Tazerouti, Samira Ihadadene

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Pyrethroids are synthetic pesticides that originated from the modification of natural pyrethrins to improve their biological activity and stability. They are a family of chiral pesticides with a large number of stereoisomers. Enantiomers of synthetic pyretroids present different insecticidal activity, toxicity against aquatic invertebrates and persistence in the environment so the development of rapid and sensitive chiral methods for the determination of different enantiomers is necessary. In this study, the separation of enantiomers of pyrethroid insecticides has been systematically studied using three commercially chiral high-performance liquid chromatography columns. Useful resolution was obtained for compounds with a variety of acid and alcohol moieties, and containing one to four chiral centres. The chromatographic behaviour of the diastereomers of some of these insecticides by using normal, polar and reversed mobile phase mode were also examined.

Keywords: pesticides, analysis, liquid chromatography, pyrethroids

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Authors: Katarzyna Zięba, Hajnalka Szentgyörgyi, Paweł Miśkowiec, Agnieszka Moos-Matysik

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Bees are effective pollinators of plants using by humans. However, there is a concern about the fate different species due to their recently decline. Pollution of the environment is described in the literature as one of the causes of this phenomenon. Due to human activities, heavy metals and aromatic hydrocarbons can occur in bee organisms in high concentrations. The presented study aims to provide information on how pollution affects bee quality, taking into account, also the biological differences between various groups of bees. Understanding the consequences of environmental pollution on bees can help to create and promote bee friendly habitats and actions. The analyses were carried out using two contamination gradients with 5 sites on each. The first, mainly heavy metal polluted gradient is stretching approx. 30km from the Bukowno Zinc smelter near Olkusz in the Lesser Poland Voivodship, to the north. The second cuts through the agglomeration of Kraków up to the southern borders of the Ojców National Park. The gradient near Olkusz is a well-described pollution gradient contaminated mainly by zinc, lead, and cadmium. The second gradient cut through the agglomeration of Kraków and end below the Ojców National Park. On each gradient, two bee species were installed: red mason bees (Osmia bicornis) and honey bees (Apis mellifera). Red mason bee is a polylectic, solitary bee species, widely distributed in Poland. Honey bees are a highly social species of bees, with clearly defined casts and roles in the colony. Before installing the bees in the field, samples of imagos of red mason bees and samples of pollen and imagos from each honey bee colony were analysed for zinc, lead cadmium, polycyclic and monocyclic hydrocarbons levels. After collecting the bees from the field, samples of bees and pollen samples for each site were prepared for heavy metal, monocyclic hydrocarbon, and polycyclic hydrocarbon analysis. Analyses of aromatic hydrocarbons were performed with gas chromatography coupled with a headspace sampler (HP 7694E) and mass spectrometer (MS) as detector. Monocyclic compounds were injected into column with headspace sampler while polycyclic ones with manual injector (after solid-liquid extraction with hexane). The heavy metal content (zinc, lead and cadmium) was assessed with flame atomic absorption spectroscopy (FAAS AAnalyst 300 Perkin Elmer spectrometer) according to the methods for honey and bee products described in the literature. Pollution levels found in bee bodies and imago body masses in both species, and proportion of sex in case of red mason bees were correlated with pollution levels found in pollen for each site and colony or trap nest. An attempt to pinpoint the most important form of contamination regarding bee health was also be undertaken based on the achieved results.

Keywords: heavy metals, aromatic hydrocarbons, bees, pollution

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Authors: Ishan Arora, Anurag Rathore

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The primary objective of this work was to study the effect of resin chemistry, pH and molarity of binding and elution buffer on aggregate removal using Cation Exchange Chromatography and find the optimum conditions which can give efficient aggregate removal with minimum loss of yield. Four different resins were used for carrying out the experiments: Fractogel EMD SO3-(S), Fractogel EMD COO-(M), Capto SP ImpRes and S Ceramic HyperD. Runs were carried out on the AKTA Avant system. Design of Experiments (DOE) was used for analysis using the JMP software. The dependence of the yield obtained using different resins on the operating conditions was studied. Success has been achieved by obtaining yield greater than 90% using Capto SP ImpRes and Fractogel EMD COO-(M) resins. It has also been found that a change in the operating conditions generally has different effects on the yields obtained using different resins.

Keywords: aggregates, cation exchange chromatography, design of experiments, monoclonal antibodies

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Authors: Pavel Shcherban, Vlad Golovanov

Abstract:

Currently, there is an active geological exploration and development of the subsoil shelf of the Kaliningrad region. To carry out a comprehensive and accurate assessment of the volumes and degree of extraction of hydrocarbons from open deposits, it is necessary to establish not only a number of geological and lithological characteristics of the structures under study, but also to determine the oil quality, its viscosity, density, fractional composition as accurately as possible. In terms of considered works, gas chromatography is one of the most capacious methods that allow the rapid formation of a significant amount of initial data. The aspects of the application of the gas chromatography method for determining the chemical characteristics of the hydrocarbons of the Kaliningrad shelf fields are observed in the article, as well as the correlation-regression analysis of these parameters in comparison with the previously obtained chemical characteristics of hydrocarbon deposits located on the land of the region. In the process of research, a number of methods of mathematical statistics and computer processing of large data sets have been applied, which makes it possible to evaluate the identity of the deposits, to specify the amount of reserves and to make a number of assumptions about the genesis of the hydrocarbons under analysis.

Keywords: computer processing of large databases, correlation-regression analysis, hydrocarbon deposits, method of gas chromatography

Procedia PDF Downloads 126

Authors: Xavier A. Conlan

Abstract:

Speed of analysis is a significant limitation to current high-performance liquid chromatography/mass spectrometry (HPLC/MS) and ultra-high-pressure liquid chromatography (UHPLC)/MS systems both of which are used in many forensic investigations. The flow rate limitations of MS detection require a compromise in the chromatographic flow rate, which in turn reduces throughput, and when using modern columns, a reduction in separation efficiency. Commonly, this restriction is combated through the post-column splitting of flow prior to entry into the mass spectrometer. However, this results in a loss of sensitivity and a loss in efficiency due to the post-extra column dead volume. A new chromatographic column format known as 'parallel segmented flow' involves the splitting of eluent flow within the column outlet end fitting, and in this study we present its application in order to interrogate the provenience of methamphetamine samples with mass spectrometry detection. Using parallel segmented flow, column flow rates as high as 3 mL/min were employed in the analysis of amino acids without post-column splitting to the mass spectrometer. Furthermore, when parallel segmented flow chromatography columns were employed, the sensitivity was more than twice that of conventional systems with post-column splitting when the same volume of mobile phase was passed through the detector. These finding suggest that this type of column technology will particularly enhance the capabilities of modern LC/MS enabling both high-throughput and sensitive mass spectral detection.

Keywords: chromatography, mass spectrometry methamphetamine, parallel segmented outlet flow column, forensic sciences

Procedia PDF Downloads 457